发布时间 : 星期四 文章中英对照-APIC 原料药厂清洁验证指南：8.0残留量检测更新完毕开始阅读
hn is the maximum deviation of the baseline within the range of 5 to 20 fold width of peak at half height. 其中：H为基线平均值的峰高
hn是基线在5-20部半峰高时峰宽范围内最大偏差
? Based on the Standard Deviation of the Response and the Slope 根据响应和斜率的标准偏差
The detection limit may be expressed by Equation 2 and the quantitation limit by Equation 3.
检查限可以采用公式2表示，定量限可以用公式3表示。
8.2.4 Determination of Recovery 回收率测定
If possible, the recovery of impurity detection for cleaning validation should be determined for the sampling and analytical methods together at least for recovery and sensitivity (Limit of Quantitation - LOQ, or Limit of Detection - LOD). This can be achieved, for example, by spiking a surface equivalent to the equipment surface (e.g. material, polish grade) with different known amounts of the impurity. The impurity can then be
recovered and analysed using the same sampling and analytical methods that will be used for the cleaning validation study. The overall results from this procedure are then compared to criteria for detection or quantitation limits as defined in ICH Q2 (R1). Validation of the limits may be achieved by the analysis of samples known to be near at the limits.
可能的话，可以针对取样方法和检验方法同时进行清洁验证中杂质检测的回收率和灵敏度（定量限-LOQ，或检测限-LOD）。例如，可以采用与设备表面材质相同的表面材料（例如，材质、粗糙度），在上面加不同已知数量的杂质，然后采用与清洁验证研究相同的方法取样并分析。再将使用该方法所得的总体结果与ICH Q2(R1)中定义的检测限或定量限标准进行比较。可对接近限度的已知样品进行分析来验证分析方法的检测限和定量限。
The measured results are then compared to the actual amount applied to the surface. The recovery is typically determined during the accuracy determination and should be reported as a percentage of the known applied amount of the impurity.
将检测结果与实际数量进行比较，用于表面残留计算。回收率一般是在准确性测试中确定，应报告为已知杂质数量的百分比。
As an example, quantitative impurity determination recoveries of ≥ 90 % are usually regarded acceptable. For cleaning validation, recoveries of ≥ 90 % do not need to be taken into account for the calculation of the true value for M. Recoveries of < 90 % must be included in the calculation for M (see Equation 4) and recoveries of < 50 % should be omitted. 例如在杂质定量测试中，回收率≥ 90 %时一般认为是可以接受的。在清洁验证中，如果回收率≥ 90 %，在M残留量真值计算中可以不需要考虑回收率；如果回收率< 90 %，则需要在M计算时加以考虑（参见公式4），如果回收率<50%，则该方法不适用。
Where: M: True value for the amount of residue remaining in the equipment after cleaning;
Mres: The measured amount of residue (sampling and then analytical measurement);
R Recovery in % divided by 100 (e.g. for 75%, 75/100 = 0.75). 公式4：
其中M：清洁后设备上残留物的数量真值 Mres：测得残留量（取样后分析测量）
R：回收率除以100（例如，对于75%即为75/100=0.75）
APIC 201405原料药厂清洁验证指南：8.0残留量检测（下）（中英文）
2014-07-11 julia翻译 蒲公英
接上部分。
8.2.5 Validation Requirements for Quantitative Testing of Impurities 杂质定量测试的验证要求
The requirements for the validation of quantitative testing of impurities according to ICH Q2 (R1) are shown in Table 2, including proposed
acceptance criteria (as an example only). Alternative acceptance criteria may be established based on sound scientific rationale.
根据ICH Q2(R1)，杂质定量检测方法的验证要求在表2中列出，包括制订的可接受标准（只是举例）。可以根据科学合理的原则制订适当的可接受标准。 It is important to note, that the summarised requirements should be used for the validation of quantitative testing for impurities during cleaning validation studies. Validation of quantitative testing for impurities is usually applied when the analytical method will be used for several specifications of the residue amount in the equipment.
重点要注意的是，在清洁验证研究中，定量检测方法验证应满足所有要求。如果分析方法将用于设备中残留量有不同的几个质量标准，则一般采用杂质定量方法验证要求。
The lowest foreseen acceptance limit is referred to as MperMin and the highest limit as MperMax in Table 2. For only one specific acceptance limit normally limit testing for impurities and the corresponding validation of the analytical method is sufficient. If the validation of quantitative testing for impurities will be used for one specific acceptance limit, then MperMin = MperMax = Mper.
最低预期可接受限度，在表2中称为MperMin，和最高限度，称为MperMax。对于只有一个特定的可接受限度，一般可以使用杂质限度测试方法，对方法只要做相应的验证即可。如果要将杂质定量方法的验证用于单一可接受限度，则MperMin = MperMax = Mper。
For the experimental work described in Table 2, the samples can be spiked with appropriate levels of the impurities (when standards are available) or compared with another well-characterised procedure (when standards are not available) to obtain the true value of the analyte concentration.